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, ethers of the present invention is claimed in Patented May 24, 1932 UNITED STATES PATENT OFFICE CHARLES E. BURKE, F WIIJ VIINGTON, DELAWARE, ASSIGNOR T0 E. I. DU PON'I DE NE- IVIOURS & COMPANY, OF WILMINGTON, DELAWARE, A CORPORATION OF DELAWARE PENTAERYTHRITE ETHERS No Drawing. Original application filed January 27, 1928, Serial No. 250,093. Divided and this application filed March 1, 1930.

This invention relates to pentaerythrite ethers.

The present application is a division of my application Serial No. 250,093, filed January 27, 1928, which resulted in Patentv No. 1,77et,500. The method of preparing the said Patent No. 1,774,500.. I The following is a specific example of one method of preparing pentaerythrite ethers.

Dissolve v775 grams of ethyl chloride in 1400 grams of benzine, and'add 400 grams of pentaerythrite (approximately 95% pure) and 520 grams of flaked-caustic soda. Heat the whole mass in a nickel autoclave forapproximately eight hours, raising the temperature to about 150 C. in the course of two hours and maintaining at about 150 C. for the remainder of the time. This reaction is carried out at a pressure of approximately 200-2l0 pounds per square inch. When the reaction is completed, allow the mass to cool over night, filter, and distill 0d the benzine from the filtrate. Then fractionate the residual material under reduced pressure, taking three fractions. The first fraction distills at a temperature of l165 C. under a pressure of 4-4 mm. mercury, the second fraction distills at l200 C. under a pressure of 50 mm., and the third fraction at 200-260 C. An analysis of these fractions indicates that the first fraction consists of approximately triethyl ether and 20% diethyl ether; the second fraction, 20% triethyl ether and 80% diethyl ether; and the third fraction 87%' diethyl ether and 12% monoethyl ether.

All three fractions are pale yellow oils and the viscosity of the third fraction is much higher than that of fractions one and two.

In place of a chloride, such as ethyl chlorlde, there may be used esters of other inorganic acids, for example, bromides, iodides,

sulfates and the like; and in place of ethyl chloride there may be used esters containlng other organic radicals, for example, me-

thyl chloride, butyl chloride, 'benzyl chloride and the like.

. These pentaerythrite ethers are, in. gen- 7' eral, useful as solvents,softeners and plasti- Serial No. 432,555.

cizers for cellulose derivatives, for example,

cellulose ethers or for cellulose esters such as cellulose nitrate, cellulose acetate and the like. The following is one method suitable for producing compositions of this nature.

Take 100 parts of a cellulose derivative, such as cellulose nitrate,.and from 2 to 60 parts of pentaerythrite ether, for example, the diethyl ether, and to this add a sufiicient quantity of a mutual solvent to form a plastic mass. Such a composition may be plasticized in a mixer followed by rolling, cakepressing and sheeting, according to the methods known to the plastic art, or the composition may be dissolved in a suitable volatile solvent and thinned to a consistency suitable for a coating composition with or without the addition of oils, resins, pigments and In testimony whereof, I affix my signa- CHARLES E. BURKE.

ture. 

